Particulate solids tube loading apparatus

ABSTRACT

Vertical tubes are expeditiously filled to a predetermined depth with flowable, particulate solids by an apparatus which comprises (a) a temporary storage reservoir for the flowable, particulate solids; (b) conveying means for supplying the temporary storage reservoir with flowable, particulate solids; (c) an overflow reservoir supported by and vertically below the temporary storage reservoir; (d) a temporary storage reservoir flow control means for regulating the quantity of flowable, particulate solids passing out of the temporary storage reservoir and into the overflow reservoir; (e) at least one vertically oriented measuring tube secured to and passing through the bottom of the overflow reservoir, which measuring tubes are (i) located beneath the temporary storage reservoir flow control means; (ii) open at their upper ends for the receipt of flowable, particulate solids which pass through the temporary storage reservoir flow control means; and (iii) restricted at their lower ends by a measuring tube flow control means, to which an outlet nozzle of variable, restricted flow area is attached; (f) screeding means for leveling the flowable, particulate solids within the measuring tube; (g) positioning means for locating the outlet nozzles above the vertical tubes to be filled with flowable, particulate solids; and (h) conveying means for removing excess flowable, particulate solids collected in the overflow reservoir.

United States Patent Hare et al. v

[ Jan. 29, 1974 PARTICULATE SOLIDS TUBE LOADING APPARATUS [75]Inventors: Thomas R. Hare, Oakland; Clifford C. Segerstrom, Lafayette,both of Calif.

[73] Assignee: Shell Oil Company, Houston, Tex.

[22] Filed: Feb. 10, 1972 [21] Appl. No.: 225,257

[52] US. Cl 141/125, 141/238, 141/264, 222/429 [51] Int. Cl 1365b l/06[58] Field of Search 222/426, 428, 429, 438; 141/250, 263, 264, 236,237, 238, 242, 244, 115, 121, 125

[5 6] References Cited UNITED STATES PATENTS 261,941 8/1882 McCrodden141/244 1,267,201 5/1918 Fleming et al 141/238 1,488,603 4/1924Kouwenhoven 141/238 2,770,395 11/1956 Sebardt 222/438 X 3,380,633 4/1968Du Bois 141/238 X Primary Examiner-l-louston S. Bell, Jr. AssistantExaminer-Charles Gorenstein Attorney, Agent, or Firm1-1oward W. Haworth[57] ABSTRACT Vertical tubes are expeditiously filled to a predetermineddepth with flowable, particulate solids by an apparatus which comprises(a) a temporary storage reservoir for the flowable, particulate solids;(b) conveying means for supplying the temporary-storage reservoir withflowable, particulate solids; (c) an overflow reservoir supported by andvertically below the temporary storage reservoir; (d) a temporarystorage reservoir flow control means for regulating the quantity offlowable, particulate solids passing out of the temporary storagereservoir and into the overflow reservoir; (e) at least one verticallyoriented measuring tube secured to and passing through the bottom of theoverflow reservoir, which measuring tubes are (i) located beneath thetemporary storage reservoir flow control means; (ii) open at their upperends for the receipt of flowable, particulate solids which pass throughthe temporary storage reservoir flow control means; and (iii) restrictedat their lower ends by a measuring tube flow control means, to which anoutlet nozzle of variable, restricted flow area is attached; (f)screeding means for leveling the flowable, particulate solids within themeasuring tube; (g) positioning means for locating the outlet nozzlesabove the vertical tubes to be filled with flowable, particulate solids;and (h) conveying means for removing excess flowable, particulate solidscollected in the overflow reservoir.

12 Claims, 3 Drawing Figures Pmmanmzsmw 3.788370 sum 10F 3 FIGQIPATENTEDJAN29 1914 3788.370-

sumanra FIG. 2

PATENTEDJANZQIQM 33 370 sum 3 or 3 FIG. 3

BACKGROUND OF THE INVENTION 1. Field of the Invention This inventionrelates to an apparatus and method for filling vertical tubes to apredetermined depth with flowable, particulate solids.

2. The Prior Art The contacting of fluids, whether as liquids, gases, ortwo-phase mixtures, with solids is a common step in modern chemicalprocesses. For example, gaseous and- /or liquid reactants areselectively converted to desired products by contacting with suitablecatalysts; product streams are purified of contaminants by contactingwith solid selective adsorbants; objectionable, ionic species areremoved from liquids by contacting with solid ion exchange resins; andgases and liquids are dried by contacting with solid desiccants. Notinfrequently, such contacting operations are accompanied by sizeableheat effects. To maintain the solid at full working capacity, and toavoid complications in the fluid being processed, the solid contactingmaterial is frequently loaded within a plurality of tubes around which asuitable heat transfer medium circulates. By appropriate manifolding,the fluid to be treated is passed through the tubes, with the generatedor required heat being removed or supplied, respectively, by thecirculating heat transfer medium.

Economies of scale have required a substantial increase in the size ofthe equipment in which such contacting operations are conducted, as wellas the number of pieces of such equipment within a particular chemicalplant. Where the fluid-solid contacting device contains thousands, oreven tens of thousands of tubes, as

is not uncommon in modern large scale chemical processes, desiredeconomies of scale can be detrimentally offset by the costs of loadingand unloading the solid contacting material from the tubes, as well asby major losses in productivity which occur during the lengthy periodthe fluid-solid contacting device is out of service for solids loadingand unloading.

In the past it was conventional to place, in effect, a funnel at theupper end of each tube to be filled and pour the flowable, particulatesolid into the individual tubes. Except for very specializedapplications, such a procedure is unacceptable today because of thelarge number of tubes which have to be filled.

To a certain extent, this funnel-filling technique has beensemi-automated by Sacken et al., US Pat. No. 3,223,490 (issued Dec. 14,1965). Sacken et al discloses a tube filling device which consists of(a) a rimmed, perforated plate which rests on the tubes to be filled,the drilled perforations corresponding to the pattem and spacing of thetubes to be filled; and (b) a fill tube (in effect, a funnel), one foreach of the many tubes to be filled, which nests in the perforated plateand extends into the tube to be filled. In operation, catalyst is dumpedonto the perforated plate, the plate is shaken, and the flowable solid,one particle at a time, passes through the fill tubes and into the tubesto be loaded. The difficulties with such a catalyst loading systeminclude: (a) inflexibility, in that a perforated plate and itsassociated fill tubes can only be used to load a fluid-solid contactingdevice tube bundle having the same number, pattern, spacing, anddiameter of tubes which correspond to the holes drilled in the rimmed,perforated plate; (b) the inordinate amount of set-up time required toslip thousands of individual fill tubes through the plate perforationsand into the upper ends of tubes to be filled; and (c) the inability toreproducibly fill the vertical tubes with strata of flowable,particulate solids comprising a mixture of two or more similar ordissimilar species, for example, catalyst mixed with varying proportionsof an inert solid diluent, where the lengths of strata in one verticaltube is duplicated in all other vertical tubes in the tube bundle.

BRIEF SUMMARY OF THE INVENTION It has now been found that vertical tubesmay be filled to a predetermined depth with flowable, particulate solidswith an apparatus which comprises (a) a temporary storage reservoir forthe flowable, particulate solids; (b) conveying means for supplying thetemporary storage reservoir with flowable, particulate sol ids; (c) anoverflow reservoir supported by and vertically below the temporarystorage reservoir; (d) a temporary storage reservoir flow control meansfor re gulating the quantity of flowable, particulate solid passing outof the temporary storage reservoir and into the overflow reservoir; (e)at least one vertically-oriented measuring tube secured to and passingthrough the bottom of the overflow reservoir, which measuring tubes are(i) located beneath the temporary storage reservoir flow control means;(ii) open at their upper ends for th receipt of flowable, particulatesolids which pass through the temporary storage reservoir flow controlmeans, and (iii) restricted at their lower ends by a measuring tube flowcontrol means, to which an outlet nozzle of variable, restricted flowarea is attached; (f) screeding means for leveling the flowable,particulate solids within the measuring tube; (g) positioning means forlocating the outlet nozzles above the vertical tubes to be filled withflowable, particulate solids; and (h) conveying means for removingexcess flowable, particulate solids collected in the overflow reservoir.

BRIEF DESCRIPTION OF THE DRAWINGS In the drawings:

FIG. 1 is a simplified diagramatic, cross sectional view of oneembodiment of the present invention, containing for purposes of clarity,three measuring tubes.

FIG. 2 is a simplified, isometric view of (a) a doctor blade assembly,which may be employed in the apparatus of the present invention as meansfor screeding flowable, particulate solids within measuring tubes; and(b) a volume-varying collar for precisely controlling the quantity offlowable, particulate solids loaded into and delivered by one dischargecycle of the measuring tubes.

FIG. 3 is a simplified elevational view illustrating the use ofsingleand multi-tube loading apparatuses in the filling of a verticallyoriented, fluid-solid contacting device tube bundle.

DETAILED DESCRIPTION OF THE DRAWINGS AND INVENTION For the purpose offacilitating an understanding of the invention, the accompanyingdrawings illustrate a preferred embodiment thereof. While one form ofthe invention is described in considerable detail in connection with thedrawings, it will be understood by those skilled in the art thatnumerous modifications can be made thereto without departing from thescope of the invention.

In FIG. 1, the flowable, particulate solids loading apparatus 19 isshown with three measuring tubes 38. The apparatus consists of atemporary storage reservoir 36, which is supplied with flowable,particulate solids via conveying means 23. Overflow reservoir 37 issuspended from and vertically below temporary storage reservoir 36. Thepassage of flowable, particulate solids from temporary storage reservoir36 to overflow reservoir 37 is regulated by temporary storage reservoirflow control means 28, for example a pinch valve, butterfly valve, orthe like. Temporary storage reservoir flow control means 28 preferablyconsists of a pneumatically-activated pinch valve. As illustrated,temporary storage reservoir flow control means 28 is actuated by air andvacuum lines 26 and 12, respectively, in conjunction with a 3-way valve.Secured to and passing through the bottom of overflow reservoir 37 is atleast one vertically oriented measuring tube 38, three of which areshown in FIG. 1. As indicated in FIG. 1, measuring tubes 38 are (a)located beneath temporary storage reservoir flow control means 28, are(b) open at their upper ends for the receipt of flowable, particulatesolids which pass through flow control means 28, and are (c) restrictedat their lower ends by measuring tube flow control means 33. Suitabledeflectors (not shown in FIG. 1) may be positioned below temporarystorage reservoir flow control means 28 and above measuring tubes 38, toassist in achieving a uniform distribution of flowable, particulatesolids to all the measuring tubes. Measuring tube flow control means 33may also be a pinch valve, a butterfly valve, or similar type of device,and as illustrated are actuated by air and vacuum lines 26 and 12,respectively, in conjunction with a 3-way valve. In a preferredembodiment, measuring tube flow control means 33 arepneumatically-actuated pinch valves. Attached to the lower end ofmeasuring tube flow control means 33 are outlet nozzles 31 of variable,restricted flow area. As used herein, variable, restricted flow areameans that the diameter of outlet nozzles 31 may be varied to match thediameter of vertical tubes 4 within a given tube bundle by installing adifferent set of such nozzles. Such outlet nozzles perferably have adiameter no larger than that of the vertical tubes to be filled.

Each loading apparatus 19 contains one or more measuring tubes 38. In apreferred embodiment of the present invention, two devices such as thatshown in FIG. 1 are used to till a vertically oriented fluid-solidcontacting device tube bundle with flowable, particulate solids. One ofthese apparatuses will have a plurality of measuring tubes 38, forexample, 4, 9, 25, 36, etc.; the number of measuring tubes 38 is notcritical for proper operation of the apparatus. The other loadingapparatus will contain a single measuring tube 38. Working inconjunction, the loading device containing the plurality of measuringtube 38 will be employed to fill most of the tubes in a fluid-solidcontacting device tube bundle. The loading apparatus containing but asingle measuring tube 38 is used to load those vertically oriented tubesaround and near the periphery of the tube bundle which are not filled bythe loading apparatus containing a plurality of measuring tubes.

Where the apparatus illustrated in FIG. 1 is to be used for loading asingle fluid-solid contacting device, measuring tubes 38 may be affixedpermanently to the bottom of overflow reservoir 37. Alternatively, if itis desired to employ the loading apparatus of the present invention in anumber of different locations, different, removable sets of measuringtubes, having variable volumes and outlet nozzle spacings, may besecured to and passed through the bottom of overflow reservoir 37.

Positioning means for locating loader 19 over tubesheet 3 and verticaltubes 4 of a fluid-solid contacting device can be varied, but as showninclude: (a) a trolley means 21 suspended from a jib crane 20, havingsuch a length and swing to permit location of outlet nozzles 31 aboveany vertical tube 4 to be filled with flowable, particulate solids; (b)swivel means 34 and lifting means 32, for rotating the apparatus in ahorizontal plane and for raising and lowering the apparatus,respectively; and at least one vertically oriented, locating detent 41,affixed to the bottom of loading apparatus 19 and extending downward atleast to the horizontal plane formed by the ends of outlet nozzles 31,which vertically oriented locating detents nest in tubes 4a adjacent tothose which are being filled with a flowable, particulate solid. Loadingapparatus 19 may be moved from one fluid-solid contacting devicelocation to another by lifting it via bale 35.

Operation of the apparatus of the present invention proceeds as follows.A predetermined amount of flowable, particulate solids enters temporarystorage reservoir 36 through conveying means 23. After temporary storagereservoir 36 has been filled, temporary storage flow control means 28 isopened, permitting flowable, particulate solids to rain down on and fillmeasuring tubes 38. The level of flowable, particulate solids withinmeasuring tubes 38 is maintained constant by removing excess materialfrom the tops thereof. This is conveniently accomplished by one or acombination of screeding means, for example, doctor blades, wipingelements, shakers, knockers, vibrators, and the like. In a preferredembodiment, a manually-, air-, or electrically-operated doctor bladeassembly 39 removes flowable, particulate solids from the top ofmeasuring tubes 38. Such solids collect at the bottom of overflowreservoir 37, and a removed therefrom, under the influence of vacuum,through conveying means 24. To assist in the removal of flowable,particulate solids from overflow reservoir 37, the bottom thereof issloped from one side to the other, as shown in FIG. 1, or alternatively,is sloped from its center to its periphery. The movement of solidscollected at the bottom of overflow reservoir 37 to conveying means 24may be further assisted by the use of a suitable vibrator 40.

After measuring tubes 38 have been filled with flowable, particulatesolids and the excess screeded therefrom, measuring tube flow controlmeans 33 are opened, thus permitting the flowable, particulate solids topass through outlet nozzles 31 into vertical tubes 4 over whichapparatus 19 has been positioned. The volume of flowable, particulatesolids which can be loaded into measuring tubes 38 will, in general, beconsiderably less than that required to completely fill vertical tubes4. Thus, it is typically necessary to fill measuring tubes 38 a numberof times and dump their contents into tubes 4. The length and diameterof measuring tubes 38 may be varied such that an integral number ofloading cycles is required to fill tubes 4. To obtain extremely fineadjustment of the volume of flowable, particulate solids which fillmeasuring tubes 38, a volumevarying collar, which fits onto the upperends of measuring tube 38 in a sleeve-like manner, may be employed. Thiscollar will have the same cross-sectional shape as that of the one ormore measuring tubes 38, that is, round, square, hexagonal, and thelike, and are secured to the measuring tube or group of tubes by wingnuts, clamps, etc. In a preferred embodiment, such volume-varying collarforms the lower portion of doctor blade assembly 39. In thisarrangement, a doctor blade is moved across the upper, open surface ofsuch volume-varying collar, filling the collar and the measuring tubesassociated therewith, and screeding excess flowable, particulate solidsfrom the tops thereof.

Where it is desirable to load a flowable, particulate solid containing asingle species into vertical tubes 4, such filling proceeds ashereinabove outlined. In certain chemical processing steps, however, itis desirable to contact the fluid with a solid comprising two or morespecies, whose concentrations vary in the direction of fluid flow.- Forexample, certain exothermic chemical reactions are conducted bycontacting a liquid or gas with a mixture of catalyst and inert soliddiluent, the concentration of catalyst increasing in the direction offlow and the concentration of inert solids decreasing. With theapparatus of the present invention, the loading of tubes with aflowable, particulate solid in strata of varying catalyst and solidinerts, is readily accomplished. Thus, measuring tubes 38 are filled anddumped a predetermined number of times with a suitable mixture ofcatalyst and solid inerts. Then, that type of flowable, particulatesolids is removed from the system and a mixture containing a differentproportion of catalyst and solid inerts is fed. In this manner, strataof varying concentration may be loaded into tubes 4.

FIG. 2 illustrates one embodiment of a screeding means for levelingsolids in and removing excess solids from the tops of measuring tubes38. Doctor blade assembly 39 comprises volume-varying collar 61, guiderails 60, and doctor blade 62. As shown in FIG. 2, volume-varying collar61 communicates with measuring tubes 38 by slipping over the lattersopen, upper ends in a sleeve-like manner; however, the manner ofsecuring the collar to the measuring tubes is not critical.

The screeding means illustrated in FIG. 2 may be employed with single ormulti-tube loaders of the present invention. By way of illustration, theassembly shown in FIG. 2 is used with a multi-tube loader containing 25measuring tubes 38 of hexagonal cross section. The volume-varying collarwill have the same shape, for example, square, hexagonal, etc. as thegroup of measuring tubes 38. The measuring tubes may be raised orlowered with respect to this collar to achieve precise control of theamount of solids loaded in and above the tubes.

After flowable, particulate solids have been distributed onto the top ofdoctor blade assembly 39, optionally with the assistance of suitabledeflectors, doctor blade 62 is pushed or pulled across the top surfaceof the volume-varying collar. This may be accomplished manually, or bysuitable pneumatic or electrical means. Such movement of the doctorblade levels the solids above the measuring tubes and removes anyexcess.

Generally, the vertical tubes (not shown in FIG. 2) to be filled withflowable, particulate solids will be arranged in a triangular or squarepattern. Accordingly, the shape formed by the periphery of the measuringtubes, taken as a unit, and their associated volumevarying collar may bedescribed as a rhombus. In a preferred embodiment, the doctor blade ismoved across the tops of the volume-varying collar in a directionparallel to one side of that rhombus. In another preferred embodiment,the leading edge of doctor blade 62, surface A-A, is arranged at anangle other than to the direction of doctor blade movement. Using such aconfiguration, flowable, particulate solids are peeled off edge B-B ofcollar 61 successively, rather than all at once, thereby avoidingjamming of the doctor blade and attrition of screeded solids.

Shearing of flowable, particulate solids during the screeding processmay be further minimized, when employing the assembly shown in FIG. 2,by supporting doctor blade 62 on guide rails 60 such that a slight gapis maintained between the upper surface of volumevarying collar 61 andthe lower surface of doctor blade 62. Generally, the spacing betweenthese two horizontal surfaces will be between about 0.1 and about 0.75inches or more. The extent of the gap between such surfaces will dependupon the particle size of the solids being processed. Suitable sweepingmeans, for example, brushes, flexible strips, and the like, extendinginto the gap, may be affixed to the underside of doctor blade 62 toinsure adequate screeding action.

FIG. 3 illustrates one embodiment of a system for filling a fluid-solidcontacting device tube bundle with flowable, particulate solids with theapparatus of the present invention. In FIG. 3, fluid-solid contactingdevice 1, containing tubes 4 which terminate at tubesheet 3, ismaintained in position by structural support 2. To expedite theinstallation and removal of the loading facilities they may be designedfor maximum portability. To this end hopper 15, primary solids receiver13, recycle solids receiver 14, their appurtenances and controls may bemounted on structural frame 16, which is designed to span and rest onthe upper cord of support structure 2. Structural frame 16 may havelifting eyes for easy handling and a catwalk for ready access to theoperating components. Loading apparatuses l8 and 19, fitted with asingle and a plurality of measuring tubes 38, respectively, have bales35 to expedite moving them. Jib cranes 20 may be readily mounted bylifting them to position and inserting hinge pins in crane brackets 11.The crane brackets will be permanently installed and, thus, two setswill be required for each fluid-solid contacting device.

As illustrated, loading of tubes 4 with a flowable, particulate solid,comprising one or more species, proceeds as follows. Starting atcontainer 6 of flowable, particulate solids delivered to the fluid-solidcontacting device site at ground level, the particles are picked up witha vacuum-activated and manually-placed, pick-up wand 7 and conveyed toprimary solids receiver 13 through line 8. Flowable, particulate solidsare conveyed to primary receiver 13 by subjecting that vessel to avacuum supplied by portable vacuum pump 5 and transmitted theretothrough line 9 and 3-way valve 29. Flowable, particulate solidsaccumulate in primary solids receiver 13 until such time as, forexample, its weight reaches a predetermined value or the solids rise toa predetermined level. At this time, a trip, which may be integral withprimary receiver 13, automatically (a) closes 3-way valve 29, thusisolating the vessel from vacuum source 5 and flow control means 51 inconveying line 8 and (b) opens primary receiver 13 to the atmospherethrough a branch in line 8 (not shown). This breaks the vacuum inprimary receiver 13, causing the receiver dump valve 52, actuated by airsupplied thru line 10 and manifold 27, to open. Accumulated flowable,particulate solids thus drop into hopper through line 53. Dump valve 52then closes and the cycle repeats itself. Should flowable, particulatesolids be dumped into hopper 15 faster than they are withdrawn and thusbuild up sufficient height to cause contact with dump valve 52, flowthrough the valve stops and the conveying cycle discontinues. Conveyingof flowable, particulate solids through line 8 continues once this levelhas fallen.

The particular method of filling hopper 15 with flowable, particulatesolids illustrated in FIG. 3 is not critical to proper operation of theapparatus of the present invention. Thus, container 6 may be elevatedand its contents dumped into hopper 15; hopper 15 may be filled atground level and thereafter positioned on structural support 16; orsolids may be conveyed from container 6 at ground level to elevatedhopper l5 pneumatically or by the use of bucket elevators,continuousflow or closed-belt conveyors, and the like. Other methods offilling hopper 15 with flowable, particulate solids will be apparent tothose skilled in the art.

From hopper 15, flowable, particulate solids gravityfeed tosingleandmulti-measuring tube loading apparatuses 18 and 19, respectively, of thepresent invention through lines 17, 22, and 23. Loading apparatuses 18and 19 are individually suspended from columnmounted jib cranes 20,which jib cranes are so positioned and of such length and swing as topermit locating either apparatus above any tube 4 in fluid-solidcontacting device'upper tubesheet 3. Loading apparatus 18 and 19 aremoved across tubesheet 3 by trolley means 21, are raised or lowered bylifting means 32, and is r0 tated in a horizontal plane by swivel means34. Both loading apparatuses may be semi-automatic and actuated by15-100 psig air supplied via lines 10 and 26. Multi-tube loader 19 willbe capable of simultaneously charging a plurality of reactor tubes 4.Single measuring tube loader 18 is employed to fill only one tube at atime, which tubes are generally located at or near the periphery oftubesheet 3. Depending on the length of tubes 4 and whether or notstrata of flowable, particulate solids of varying concentration are tobe loaded therein, measuring tubes 38 of variable volume may beemployed. These measuring tubes may be fastened within the machine bystuds and nuts, and thus be readily removable. As discussed inconnection with FIGS. 1 and 2, the length, and, as a result, the volumeof the measuring tubes may be adjusted by the use of a volume-varyingcollar, which fits onto the upper ends of the measuring tubes in asleeve-like manner (not shown in FIG. 3) to assure the precise volume oftheir charge. By the use of suitable control elements, loadingapparatuses I8 and 19 may be programmed to give any number of dischargesper actuation, for example, from 1 to 10, by setting a cycle counterdial.

Once the movement of flowable, particulate solids to loading apparatuses18 and 19 has begun, actual loading of vertical tubes 4 may beinitiated. First, the loading apparatus will be positioned over tubes 4to be filled and lowered to within about one-eighth inch of the top oftubesheet 3. Then, temporary reservoir flow control means 28, preferablypneumatically actuated pinch valves, will momentarily open and deposit apredetermined volume of flowable, particulate solids in, and on,measuring tubes 38, which will then be screeded, for example, by doctorblade assembly 39 as shown in FIG.

' 2. Thereafter, measuring tube flow control means 33,

preferably pneumatically actuated pinch valves, will open andstarve-feed the charge of flowable, particulate solids through outlet.nozzles 31 into tubes 4. This loading cycle may be automaticallyrepeated for as many times as has been set on a cycle counter. After oneset of tubes has been loaded, the apparatus will be raised, moved to itsnext location, and the procedure repeated.

As noted hereinabove, during each cycle of loading, a portion offlowable, particulate solids will be screeded from the top of themeasuring tubes 38. These solids will accumulate within overflowreservoir 37 until, at the operators discretion, it is returned tohopper 15 through line 24, flow control means 30, line 54, recyclesolids reservoir 14, air-actuated dump valve 52 and line 55. This isaccomplished by pneumatically closing flow control means 29 therebysubjecting recycle receiver 14 to a vacuum, and opening flow controlmeans 30. The bottom of recycle solids receiver 14 may be locatedsomewhat higher than that of primary solids receiver 13, so that dumpvalve 52 therein will never be contacted by flowable, particulate solidsaccumulating in hopper l5, and, consequently, be shut off.

Locating a loading apparatus of the present invention and maintainingits position during the actual loading cycle will be assisted bylocating detents 41, which nest in tubes adjacent to those being filled.

Normally it will be advisable to consider the placement of tubes 4terminating at tubesheet 3. This will assist in determining the optinumnumber of measuring tubes with which loading apparatus 19 is to beequipped, as well as in determining the optimal pattern by which tubes 4are to be loaded. Simultaneously with, or following, the loading ofpluralities of tubes 4 by multi-measuring tube loader 19, single tubeloader 18 is employed to fill tubes located on and near the periphery oftubesheet 3. Perforations in tubesheet 3 corresponding to tie rods,plugged tubes, or' tubes to be hand-packed bacuse they containthermocouples or otherwise, are covered with a suitable protectivedevice, for example, a simple plate, while apparatuses 18 and 19 arebeing used to fill tubes 4. Any excess, flowable, particulate solidsspilled onto tubesheet 3 are removed, for example by a suitable vacuumline, before the fluid-solid contacting device is started up.

When the particular processing operation effected in fluid-solidcontacting device 1 requires that tubes 4 be filled with strata offlowable, particulate solids containing two or more species in varyingconcentrations, hopper 15 may be drained of solids by disconnectinglines 22 and 23 at loading apparatuses 18 and 19 and allowing the solidsto fall into a suitable container through these lines. After loadingmachines 18 and 19 have also been emptied of solids, filling of hopper15 with the material required in the next stratum will be started. Wheretubes 4 are to be filled with strata of differing concentration andlength, longer or shorter measuring tubes, as appropriate, may beinstalled in loading apparatuses 18 and 19 concurrently with the removalof flowable, particulate solids from the system. Where fluid-solidcontacting device 1 is to be employed in a horizontal configuration, itmay be loaded as hereinabove indicated and thereafter positioned.

We claim as our invention:

1. Apparatus for filing a vertical tube to a predetermined depth with aflowable, particulate solid which comprises a. a temporary storagereservoir for flowable, particulate solids;

b. conveying means for supplying the temporary storage reservoir withflowable, particulate solids;

c. an overflow reservoir supported by and vertically below the temporarystorage reservoir;

d. a temporary storage reservoir flow control means for regulating thequantity of flowable, particulate solids passing out of the temporarystorage reservoir and into the overflow reservoir;

e. at least one vertically oriented measuring tube secured to andpassing through the bottom of the overflow reservoir, which measuringtubes are i. located beneath the temporary storage reservoir flowcontrol means;

ii. open at their upper ends for the receipt of flowable, particulatesolids which pass through the temporary storage reservoir flow controlmeans; and

iii. restricted at their lower ends by a measuring tube flow controlmeans, which comprises an outlet nozzle of variable, restricted flowarea;

f. screeding means for leveling the flowable, particulate solids withinthe measuring tube;

g. positioning means for locating the outlet nozzle above the verticaltubes to be filled with flowable, particulate solids; and

h. conveying means for removing excess flowable,

particulate solids collected in the overflow reservoir.

2. The apparatus of claim 1 wherein the temporary storage reservoir flowcontrol means and the measuring tube flow control means comprise pinchvalves.

3. The apparatus of claim 1 wherein the screeding means comprises adoctor blade.

4. The apparatus of claim 1 wherein the positioning means comprise a. inascending order above the temporary storage reservoir i. swivel andlifting means, for rotating the apparatus in a horizontal plane, andraising and lowering the apparatus, respectively; and ii. a trolleymeans suspended from a jib crane of such length and swing to permitlocation of the outlet nozzle above a vertical tube to be filled withflowable, particulate solids; and b. at least one vertically-oriented,locating detent, af-

fixed to the bottom of the apparatus and extending downward at least tothe horizontal plane formed by the ends of the outlet nozzles, whichvertically oriented locating detents nest in tubes adjacent to thosebeing filled with flowable, particulate solids. 5. The apparatus ofclaim 1 wherein the bottom of the overflow reservoir, to which themeasuring tubes are sesured and through which they pass, is sloped fromone side to its opposite side.

6. The apparatus of claim 1 wherein the bottom of the overflowreservoir, to which the measuring tubes are secured and through whichthey pass, is sloped from its center to its outer edges.

7. The apparatus of claim 1 wherein the variable, restricted flow areaof the outlet nozzle attached to the measuring tube flow control meanshas a diameter no larger than that of the vertical tube to be filledwith flowable, particulate solids.

8. In combination with the apparatus of claim 1, a volume-varyingcollar, which fits onto the upper ends of the measuring tubes in asleeve like manner, said measuring tubes being raised or lowered withrespect to the collar to achieve precise control of the length and thevolume of the measuring tubes.

9. The apparatus of claim 1 wherein the measuring tubes are removablefrom the overflow reservoir.

10. The apparatus of claim 1 wherein a single, vertically orientedmeasuring tube is secured to and passes through the bottom of theoverflow reservoir.

11. The apparatus of claim 1 wherein a plurality of measuring tubes,measuring tube flow control means, and outlet nozzles are secured to andpass through the bottom of the overflow reservoir, which outlet nozzlesare arranged in a pattern identical to that of the vertical tubes to befilled with flowable, particular solids.

12. Apparatus for filling vertical tubes to a predetermined depth with aflowable, particulate solid which comprises a. two temporary storagereservoirs for flowable, particulate solids;

b. conveying means for supplying the temporary storage reservoirs withflowable, particulate solids;

c. two overflow reservoirs supported by and vertically below the twotemporary storage reservoirs;

d. a temporary storage reservoir flow control means for regulating thequantity of flowable, particulate solids passing out of the temporarystorage reservoir and into the overflow reservoir;

e. one vertically oriented measuring tube secured to and passing throughthe bottom of one overflow reservoir and a plurality of measuring tubessecured to and passing through the bottom of the other overflowreservoir, which measuring tube and tubes are i. located beneath therespective temporary storage reservoir flow control means;

ii. open at their upper ends for the receipt of flowable, particulatesolids which pass through the temporary storage reservoir flow controlmeans; and

iii. restricted at their lower ends by a measuring tube flow controlmeans, which comprises an outlet nozzle of variable, restricted flowarea;

f. screeding means for leveling the flowable, particulate solids withinthe measuring tube;

g. positioning means for locating the outlet nozzles above the verticaltubes to be filled with flowable, particulate solids; and

h. conveying means for removing excess flowable,

particulate solids collected in the overflow reservoirs.

1. Apparatus for filing a vertical tube to a predetermined depth with aflowable, particulate solid which comprises a. a temporary storagereservoir for flowable, particulate solids; b. conveying means forsupplying the temporary storage reservoir with flowable, particulatesolids; c. an overflow reservoir supported by and vertically below thetemporary storage reservoir; d. a temporary storage reservoir flowcontrol means for regulating the quantity of flowable, particulatesolids passing out of the temporary storage reservoir and into theoverflow reservoir; e. at least one vertically oriented measuring tubesecured to and passing through the bottom of the overflow reservoir,which measuring tubes are i. located beneath the temporary storagereservoir flow control means; ii. open at their upper ends for thereceipt of flowable, particulate solids which pass through the temporarystorage reservoir flow control means; and iii. restricted at their lowerends by a measuring tube flow control means, which comprises an outletnozzle of variable, restricted flow area; f. screeding means forleveling the flowable, particulate solids within the measuring tube; g.positioning means for locating the outlet nozzle above the verticaltubes to be filled with flowable, particulate solids; and h. conveyingmeans for removing excess flowable, particulate solids collected in theoverflow reservoir.
 2. The apparatus of claim 1 wherein the temporarystorage reservoir flow control means and the measuring tube flow controlmeans comprise pinch valves.
 3. The apparatus of claim 1 wherein thescreeding means comprises a doctor blade.
 4. The apparatus of claim 1wherein the positioning means comprise a. in ascending order above thetemporary storage reservoir i. swivel and lifting means, for rotatingthe apparatus in a horizontal plane, and raising and lowering theapparatus, respectively; and ii. a trolley means suspended from a jibcrane of such length and swing to permit location of the outlet nozzleabove a vertical tube to be filled with flowable, particulate solids;and b. at least one vertically-oriented, locating detent, affixed to thebottom of the apparatus and extending downward at least to thehorizontal plane formed by the ends of the outlet nozzles, whichvertically oriented locating detents nest in tubes adjacent to thosebeing filled with flowable, particulate solids.
 5. The apparatus ofclaim 1 wherein the bottom of the overflow reservoir, to which themeasuring tubes are sesured and through which they pass, is sloped fromone side to its opposite side.
 6. The apparatus of claim 1 wherein thebottom of the overflow reservoir, to which the measuring tubes aresecured and through which they pass, is sloped from its center to itsouter edges.
 7. The apparatus of claim 1 wherein the variable,restricted flow area of the outlet nozzle attached to the measuring tubeflow control means has a diameter no larger than that of the verticaltube to be filled with flowable, particulate solids.
 8. In combinationwith the apparatus of claim 1, a volume-varying collar, which fits ontothe upper ends of the measuring tubes in a sleeve like manner, saidmeasuring tubes being raised or lowered with respect to the collar toachieve precise control of the length and the volume of the measuringtubes.
 9. The apparatus of claim 1 wherein the measuring tubes areremovable from the overflow reservoir.
 10. The apparatus of claim 1wherein a single, vertically oriented measuring tube is secured to andpasses through the bottom of the overflow reservoir.
 11. The apparatusof claim 1 wherein a plurality of measuring tubes, measuring tube flowcontrol means, and outlet nozzles are secured to and pass through thebottom of the overflow reservoir, which outlet nozzles are arranged in apattern identical to that of the vertical tubes to be filled withflowable, particular solids.
 12. Apparatus for filling vertical tubes toa predetermined depth with a flowable, particulate solid which comprisesa. two temporary storage reservoirs for flowable, particulate solids; b.conveying means for supplying the temporary storage reservoirs withflowable, particulate solids; c. two overflow reservoirs supported byand vertically below the two temporary storage reservoirs; d. atemporary storage reservoir flow control means for regulating thequantity of flowable, particulate solids passing out of the temporarystorage reservoir and into the overflow reservoir; e. one verticallyoriented measuring tube secured to and passing through the bottom of oneoverflow reservoir and a plurality of measuring tubes secured to andpassing through the bottom of the other overflow reservoir, whichmeasuring tube and tubes are i. located beneath the respective temporarystorage reservoir flow control means; ii. open at their upper ends forthe receipt of flowable, particulate solids which pass through thetemporary storage reservoir flow control means; and iii. restricted attheir lower ends by a measuring tube flow control means, which comprisesan outlet nozzle of variable, restricted flow area; f. screeding meansfor leveling the flowable, particulate solids within the measuring tube;g. positioning means for locating the outlet nozzles above the verticaltubes to be filled with flowable, particulate solids; and h. conveyingmeans for removing excess flowable, particulate solids collected in theoverflow reservoirs.